CN115444825B - Preparation method of radix paeoniae alba and liquorice soup freeze-dried powder - Google Patents
Preparation method of radix paeoniae alba and liquorice soup freeze-dried powder Download PDFInfo
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- CN115444825B CN115444825B CN202210636060.7A CN202210636060A CN115444825B CN 115444825 B CN115444825 B CN 115444825B CN 202210636060 A CN202210636060 A CN 202210636060A CN 115444825 B CN115444825 B CN 115444825B
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- CN
- China
- Prior art keywords
- licorice
- freeze
- radix paeoniae
- dried powder
- paeoniae alba
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/19—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles lyophilised, i.e. freeze-dried, solutions or dispersions
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
- A61K36/484—Glycyrrhiza (licorice)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/65—Paeoniaceae (Peony family), e.g. Chinese peony
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- A—HUMAN NECESSITIES
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- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/71—Ranunculaceae (Buttercup family), e.g. larkspur, hepatica, hydrastis, columbine or goldenseal
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Abstract
The invention provides a preparation method of radix paeoniae alba and licorice decoction freeze-dried powder, belonging to the technical field of traditional Chinese medicine preparations, wherein the preparation method is to add radix paeoniae alba into an ethanol water solution with concentration of 80-90 wt%, adjust the pH value, soak, and then cover and decoct the radix paeoniae alba to obtain radix paeoniae alba liquid medicine; adding Glycyrrhrizae radix into water, adjusting pH, soaking, decocting, and filtering to obtain Glycyrrhrizae radix liquid medicine; mixing radix Paeoniae alba liquid medicine and Glycyrrhrizae radix liquid medicine, concentrating, and lyophilizing to obtain the radix Paeoniae and Glycyrrhrizae radix soup lyophilized powder. The 17 effective components in the Paeonia lactiflora and licorice decoction prepared by the invention are improved compared with the decoction method in the classical prescription, and the curative effect of the Paeonia lactiflora and licorice decoction can be effectively improved.
Description
Technical Field
The invention relates to preparation of traditional Chinese medicine freeze-dried powder, in particular to a preparation method of peony and licorice soup freeze-dried powder.
Background
The Paeonia lactiflora and licorice decoction is the 6 th prescription in the category of classical names (first batch). The original text comes from the treatise on typhoid fever (Han. Zhang Zhongjing), and is described as "the typhoid fever pulse is superficial, spontaneous sweating, frequent urination, vexation, slight aversion to cold, foot contracture. … … for foot warming, it is combined with Paeonia radix Glycyrrhizae decoction to stretch the foot. The original text records the prescription composition of four or two of radix paeoniae alba and radix glycyrrhizae respectively, and the prescription composition is roasted. The two medicines are boiled with three liters of water, one liter is boiled, five times are combined, dregs are removed, and the medicines are taken after being separated into temperature. "according to the literature and examination data, the modern application dosage and processed product are determined by research: white peony root 12g, water-roasted licorice 12g. Has effects of softening liver, relaxing muscles and tendons, relieving spasm and pain. Can be used for treating yin blood, body fluid deficiency, and malnutrition of tendons and vessels, and can also be used for preventing heart disease and treating varicosis.
The original text records that the decoction method is that the two medicines are decocted by three liters of water, one liter of five medicines are decocted, and the decoction is calculated according to the fact that the modern volume is 200mL and the modern volume is 20mL by one liter of Chinese instead of one liter, the Chinese herbaceous peony and licorice decoction is converted into the two medicines in the modern preparation method, 600mL of water is added, and the decoction is decocted until the liquid medicine is 300mL. However, the method is time-consuming, inconvenient to take, and unfavorable for quality control and use.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of freeze-dried powder of paeonia lactiflora and licorice decoction.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the freeze-dried powder of the peony and licorice soup is characterized by comprising the following steps of:
adding white paeony root into an ethanol water solution with the concentration of 80-90 wt%, regulating the pH value to 6.0-6.5, soaking, covering and decocting, and filtering to obtain white paeony root liquid medicine;
adding licorice into water, regulating pH to 7.2-7.5, soaking, decocting, filtering to obtain licorice liquid;
mixing radix Paeoniae alba liquid medicine and Glycyrrhrizae radix liquid medicine, concentrating, and lyophilizing to obtain the radix Paeoniae and Glycyrrhrizae radix soup lyophilized powder.
Further, the dosage of the ethanol aqueous solution is 7 to 8 times of the weight of the white paeony root; the water consumption is 8-10 times of the weight of the liquorice.
Further, the white paeony root is decocted for 1.5 to 2 hours by slow fire; the liquorice is decocted for 2-3 hours by slow fire.
Further, the soaking time of the white paeony root and the liquorice is 0.5-1 h.
Further, the concentration is carried out under the conditions of 60-80 ℃ and-0.08 to-0.1 MPa.
Further, after concentration and before freeze drying, the total weight ratio of the concentrated solution to the white paeony root and the liquorice is 1.8-2.2: 1.
further, the freeze drying is to pre-freeze at-30 to-45 ℃ for at least 60min, and then vacuum drying at-40 to-70 ℃ for at least 12h.
Further, the vacuum degree of vacuum drying is less than 100Pa.
Further, the weight ratio of the white paeony root to the liquorice is 1:1.
the preparation method of the freeze-dried powder of the peony and licorice soup has the beneficial effects that:
according to the invention, the 17 most main effective components in the peony and licorice soup are detected, and the different characteristics of the radix paeoniae alba and the licorice are utilized, and different solvents are adopted for extraction respectively, so that the content of the 17 effective components in the finally prepared freeze-dried powder of the peony and licorice soup can be effectively increased;
according to the invention, effective components such as gallic acid, isoliquiritigenin, paeonol, albiflorin, paeoniflorin, albiflorin B, benzoic acid, naringenin and benzoylpaeoniflorin and the like extracted from radix paeoniae alba are examined, and apigenin, glycyrrhizin, formononetin, neoglycyrrhizin, 3' -deoxidized Su Mutong A, isoliquiritigenin, glycyrrhizin and glycyrrhizic acid extracted from radix paeoniae alba are extracted under different extraction conditions by selecting extraction solvents which are more suitable for radix paeoniae alba and radix glycyrrhizae, so that the extraction quantity of the effective components is effectively increased;
17 effective components in the radix paeoniae alba and licorice decoction prepared by the invention are improved compared with the decoction method in the classical prescription, so that the curative effect of the radix paeoniae alba and licorice decoction can be effectively improved;
according to the invention, through selecting proper concentration and freeze-drying processes, the freeze-dried powder is prepared under the condition of ensuring that the content of the effective components is not reduced as much as possible, so that the convenience of storage and administration is improved;
the invention has simple production process and low solvent consumption, can save the time of concentration and freeze-drying, and reduces the production cost.
Drawings
FIG. 1 is a high performance liquid chromatogram of lyophilized powder of radix Paeoniae and Glycyrrhrizae radix decoction in embodiment 1 of the invention;
fig. 2 is a high performance liquid chromatogram of the freeze-dried powder of the peony and licorice decoction in comparative example 1 of the present invention.
Detailed Description
The following description of the technical solution in the embodiments of the present invention is clear and complete. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Example 1 preparation method of Paeonia lactiflora and Glycyrrhiza decoction lyophilized powder
The embodiment is a preparation method of radix paeoniae alba and liquorice soup freeze-dried powder, and the specific synthetic process comprises the following steps:
1) Taking 12g of white paeony root, adding 8 times of 85wt% ethanol water solution (96 g), dripping a small amount of 10wt% hydrochloric acid to adjust the pH value to 6.5, soaking for 1h, adding a cover, decocting with slow fire for 1.5h, and filtering by a 200-mesh nylon sieve at normal pressure to obtain white paeony root liquid medicine;
2) Adding water (108 g) which is 9 times of licorice into 12g of licorice, dropwise adding a small amount of 10wt% sodium hydroxide aqueous solution to adjust the pH value to 7.4, soaking for 1h, directly decocting with slow fire for 2.5h without covering, and filtering by a 200-mesh nylon sieve at normal pressure to obtain licorice liquid medicine;
3) Mixing radix Paeoniae alba liquid medicine and Glycyrrhrizae radix liquid medicine, concentrating under reduced pressure at 70deg.C and-0.1 MPa, stopping concentrating until the obtained concentrated solution is 48g, transferring into freeze dryer, pre-freezing at-35deg.C for 60min, cooling to-50deg.C, vacuum drying at-50deg.C under vacuum degree less than 100Pa for 12 hr, and pulverizing to obtain 7.47g radix Paeoniae Glycyrrhrizae radix decoction lyophilized powder marked as M1. The obtained radix paeoniae alba and licorice decoction freeze-dried powder is dry paste powder of radix paeoniae alba and licorice decoction, and the dry paste rate is 32.25%.
The content of 17 effective components of the freeze-dried powder M1 of the peony and licorice decoction is measured by high performance liquid chromatography, the obtained chromatogram is shown in figure 1, and the specific measuring method is as follows:
b1 Preparation of test solution and reference solution
b11 Preparation of test sample solution
0.1g of the freeze-dried powder M1 (namely M) of the peony and licorice decoction is precisely weighed out Radix paeoniae alba =0.1 g), put into a 10mL measuring flask, add 0.5wt% sodium hydroxide aqueous solution to dissolve and dilute to scale, ultrasound for 100min under 40kHz and 300W, cool to obtain dissolution liquid;
precisely transferring 1mL of the dissolution liquid, placing the dissolution liquid in a 5mL measuring flask, diluting with ethanol, fixing the volume to a scale, and shaking uniformly to obtain a sample solution; at this time, the freeze-drying of 0.1g of Paeonia lactiflora and Glycyrrhiza decoction corresponds to the volume of the prepared test solution of V Test on test ＝50mL。
b12 Preparation of control stock solution
The preparation method comprises the steps of respectively taking appropriate amounts of gallic acid, isoliquiritigenin, paeonol, albiflorin, paeoniflorin B, benzoic acid, naringenin, benzoylpaeoniflorin, apioglycyrrhizin, glycyrrhizin, formononetin, neoglycyrrhizin, 3' -deoxy Su Mutong A, isoliquiritigenin, glycyrrhizin and glycyrrhizic acid reference substances, precisely weighing, dissolving and diluting with 70wt% ethanol aqueous solution to obtain a solution with concentration of 135.274 mug/mL (gallic acid), 40.125 mug/mL (concentration of isoliquiritigenin), 0.415 mug/mL (concentration of paeonol), 86.249 mug/mL (concentration of paeoniflorin), 318.615 mug/mL (concentration of paeoniflorin), 431.743 mug/mL (concentration of apioglycyrrhizin), 95.893 mug/mL (concentration of glycyrrhizin), 6.124 mug/mL (concentration of paeoniflorin B), 4.320 mug/mL (concentration of benzoic acid), 10.410 mug/mL (concentration of naringin), 7.920 muginein/mL (concentration of 3832 muginein), stock solution with concentration of 3 muginein (concentration of 3 muginein/mL (concentration of 3 muginein), and 37 muginein (concentration of 3.3737 muginein) of 3 muginein (concentration of 3 muginein).
b13 Standard series solutions of different concentrations of reference substances
Precisely measuring 1, 2, 4, 5, 8 and 10mL of reference substance stock solutions respectively, placing the reference substance stock solutions in 50, 20, 10 and 10mL measuring flasks, and fixing the volumes by using 70wt% ethanol water solution to serve as reference substance standard series solutions with different concentrations, wherein the concentrations of different chemical components are shown in Table 1.
b2 High performance liquid chromatography detection
b21 Taking reference standard series solutions with different concentrations, and performing high performance liquid chromatography detection under the above chromatographic conditions to obtain peak areas of corresponding chemical components measured according to the concentrations, wherein the specific peak areas are shown in Table 1.
Table 1A list of test results for Standard series solutions of reference substances at different concentrations
Wherein, the high performance liquid chromatography conditions of the standard solution of the detection reference substance are as follows:
chromatographic column: YMC-Triart C18 (5 μm, 4.6X1250 mm);
mobile phase: acetonitrile (a) -0.1wt% formic acid in water (B);
elution procedure: 0-5 min,5% -13% mobile phase A,95% -87% mobile phase B;
5-15 min,13% -23% mobile phase A,87% -77% mobile phase B;
15-40 min,23% -50% mobile phase A,77% -50% mobile phase B;
40-55 min,50% -100% mobile phase A,50% -0% mobile phase B;
55-55.01 min,100% -5% mobile phase A,0% -95% mobile phase B;
55.01-65 min,5% mobile phase A,95% mobile phase B.
Flow rate: 0.60mL/min;
column temperature: 35 ℃;
detection wavelength: 230nm;
sample injection amount: 5. Mu.L.
And drawing a standard curve corresponding to the different chemical components according to the concentrations of the different chemical components and the peak areas measured according to the concentrations of the corresponding chemical components, wherein the concentrations of the different chemical components are taken as an abscissa (namely x, the unit is mu g/mL), and the peak areas measured according to the concentrations of the corresponding chemical components are taken as an ordinate (namely y).
The standard curves drawn with the reference standard series solutions of different concentrations are as follows:
the standard curve corresponding to gallic acid is y=7893.9x+10.438, r 2 ＝1.000；
The standard curve corresponding to isoliquiritigenin is y=9517x+8090.5, R 2 ＝0.9999；
Paeonol has standard curve of y= 874711x-597.18, R 2 ＝1.000；
The standard curve corresponding to the paeoniflorin is y=4789 x-1561.8, R 2 ＝0.9995；
The standard curve corresponding to paeoniflorin is y=12301x+21868, R 2 ＝0.9996；
The standard curve corresponding to apigenin is y= 8142.2x-3638.1, R 2 ＝0.9993；
The standard curve corresponding to glycyrrhizin is y=19786x+11017, R 2 ＝0.9996；
The standard curve corresponding to the albino B is y=47442x+629.14, r 2 ＝0.9996；
Benzoic acid corresponds to a standard curve y= 106956x-899.14, r 2 ＝1.000；
Naringenin has a standard curve of y= 40543x-1700.9, R 2 ＝0.9996；
The standard curve corresponding to formononetin is y= 40417x-1051.9, R 2 ＝0.9994；
The standard curve corresponding to the new glycyrrhizin is y= 61161x-1294, R 2 ＝0.9998；
The standard curve corresponding to 3' -deoxy Su Mutong a is y=49390x+298.4, r 2 ＝0.9999；
Isoliquiritigenin has a standard curve of y= 28818x-272.07, R 2 ＝0.9998；
The standard curve corresponding to the glycyrrhizin isy＝16997x+371.77，R 2 ＝0.9998；
The standard curve corresponding to the benzoylpaeoniflorin is y= 1684.4x-587.75, R 2 ＝0.9999；
The standard curve corresponding to glycyrrhizic acid is y=5868.1x+14514, R 2 ＝0.9995。
b23 Taking the sample solution, performing high performance liquid chromatography detection under the above chromatographic conditions to obtain peak areas corresponding to different chemical components contained in the sample solution, substituting the peak areas of the corresponding chemical components into corresponding standard curves to obtain the concentration (C) of the corresponding chemical components in the sample solution Test-corresponding chemical composition )。
And then the concentration (C) of the corresponding chemical component in the sample solution Test-corresponding chemical composition ) Multiplied by the total volume of the prepared test solution (V Test on test =50 mL) divided by the amount of the freeze-dried powder of the peony and licorice decoction used for preparing the test solution (m Radix paeoniae alba =0.1 g), i.e. the content of the corresponding chemical component in the peony and licorice soup, that is to say the content of the corresponding chemical component in the peony and licorice soup= (C) Para-corresponding chemical composition ×V Test on test )/m Radix paeoniae alba 。
In the case of glycyrrhizic acid, the peak area (A) Para-glycyrrhizic acid = 436727) substituting the standard curve corresponding to glycyrrhizic acid, and calculating to obtain the concentration (C) Glycyrrhizinic acid ＝71.95μg/mL)；
Content of glycyrrhizic acid in Paeonia lactiflora and Glycyrrhiza decoction= (C) Para-glycyrrhizic acid ×V I-glycyrrhizic acid )/m Radix paeoniae alba ＝65.134μg/mL×50mL/0.1g＝29606.5μg/g＝35.98mg/g。
In the embodiment, the paeonia lactiflora decoction M1 contains 2.074mg/g of gallic acid, 3.321mg/g of isoliquiritigenin, 0.0058mg/g of paeonol, 1.369mg/g of paeoniflorin, 52.71mg/g of paeoniflorin, 0.1023mg/g of paeoniflorin B, 0.0676mg/g of benzoic acid, 0.1529mg/g of naringenin, 5.524mg/g of benzoylpaeoniflorin, 28.64mg/g of apioglycyrrhizin, 26.19mg/g of glycyrrhizin, 0.1217mg/g of formononetin, 0.1034mg/g of neoglycyrrhizin, 0.1426mg/g of 3' -deoxysappan ketone A, 0.2312mg/g of isoliquiritigenin, 0.2628mg/g of glycyrrhizin and 47.98mg/g of glycyrrhizic acid.
Equivalently, the analysis of the components in the preparation of the peony and licorice decoction M1 in this example is specifically shown in the following table:
TABLE 2 list of results of active ingredients in Paeonia lactiflora and Glycyrrhiza decoction
| Active ingredient | Content of active ingredient (mg/g) | Total amount of each active ingredient | Extraction efficiency (%) |
| Gallic acid | 2.074 | 16.05276 | 0.134 |
| Isoglycyrrhizin | 3.321 | 25.70454 | 0.214 |
| Paeonol | 0.0058 | 0.044892 | 0.0004 |
| Albiflorin | 1.369 | 10.59606 | 0.0883 |
| Paeoniflorin | 52.71 | 407.9754 | 0.34 |
| Apiose glycyrrhizin | 28.64 | 221.6736 | 1.85 |
| Liquiritigenin | 26.19 | 202.7106 | 1.69 |
| Albiflorin B | 0.1023 | 0.791802 | 0.0066 |
| Benzoic acid | 0.0676 | 0.523224 | 0.0044 |
| Naringenin | 0.1529 | 1.183446 | 0.0099 |
| Formononetin-like element | 0.1217 | 0.941958 | 0.0078 |
| Novel glycyrrhizin | 0.1034 | 0.800316 | 0.0067 |
| 3' -deoxy Su Mutong A | 0.1426 | 1.103724 | 0.0092 |
| Isoliquiritigenin | 0.2312 | 1.789488 | 0.0149 |
| Liquiritigenin | 0.2628 | 2.034072 | 0.017 |
| Benzoyl paeoniflorin | 5.524 | 42.75576 | 0.356 |
| Glycyrrhizic acid | 47.98 | 371.3652 | 2.32 |
EXAMPLES 2-6 preparation method of Paeonia lactiflora and Glycyrrhiza decoction lyophilized powder
Examples 2 to 6 are respectively a preparation method of radix paeoniae alba and licorice decoction freeze-dried powder, and the steps are basically the same as those of example 1, except that the raw material dosage and the technological parameters are different, and the specific details are shown in table 3:
table 3 list of process parameters in examples 2 to 5
The other parts of examples 2 to 6 are the same as in example 1.
Determination of Experimental example 1 content
Comparative examples 1 to 6 are comparative experiments of the preparation process of the freeze-dried powder of the peony and licorice decoction in example 1, and the difference between the radix paeoniae alba and the licorice is that the same batch of medicinal materials is taken from example 1, and the difference is that:
in comparative example 1, four or two of the Chinese herbaceous peony and licorice root are processed according to the description of typhoid fever. The two above two medicines are boiled with three liters of water, one liter of five medicines is removed, the dregs are separated, then the mixed liquor of white paeony root and liquorice is prepared, and then the mixed liquor is concentrated and freeze-dried by the method in the example 1 to prepare 5.04 white paeony root and liquorice soup freeze-dried powder, wherein the dry paste rate is 21.00 percent, and the white paeony root and liquorice soup freeze-dried powder DM1 contains 1.614mg/g gallic acid, 0.8241mg/g isoliquiritigenin, 0.0045mg paeonol, 0.8632mg of paeoniflorin, 41.44mg/g paeoniflorin, 0.0678mg/g paeoniflorin, 0.0459mg/g benzoic acid, 0.1042mg/g naringenin, 3.512mg/g benzoylpaeoniflorin, 24.12mg/g apigenin, 19.69mg/g glycyrrhizin, 0.0798mg formononetin, 0.0657mg/g neoglycyrrhizin, 3' -deoxidized Su Mutong A0.0869 mg/g, 0.1534mg isoliquiritigenin and 0.1856.63 mg liquorice.
1.614mg/g of gallic acid, 0.8241mg/g of isoliquiritigenin, 0.0045mg/g of paeonol, 0.8632mg/g of paeoniflorin, 41.44mg/g of paeoniflorin, 0.0678mg/g of paeoniflorin B, 0.0459mg/g of benzoic acid, 0.1042mg/g of naringenin, 3.512mg/g of benzoylpaeoniflorin, 24.12mg/g of apigenin, 19.69mg/g of liquiritin, 0.0798mg/g of formononetin, 0.0657mg/g of neoglycyrrhizin, 0.0869mg/g of 3' -deoxy Su Mutong A, 0.1534mg/g of isoliquiritigenin, 0.1856mg/g of liquiritigenin and 29.61mg/g of glycyrrhizic acid.
In the step 1) in the comparative example 2, only 85wt% of ethanol aqueous solution is replaced by 100% ethanol, the obtained 6.86g of radix paeoniae alba and licorice soup freeze-dried powder is marked as DM2, the dry paste rate is 28.58%, and the radix paeoniae alba and licorice soup freeze-dried powder DM2 contains 2.121mg/g gallic acid, 3.314mg/g isoliquiritigenin, 0.0062mg/g paeonol, 0.657mg/g albiflorin, 34.24mg/g paeoniflorin, 0.8793mg/g paeoniflorin, 0.0423mg/g benzoic acid, 0.1293mg/g naringenin, 4.912mg/g benzoyl paeoniflorin, 28.38mg/g apigenin, 26.27mg/g glycyrrhizin, 0.1224mg/g formononetin, 0.1021mg/g neoglycyrrhizin, 3' -deoxidized Su Mutong A0.1409 mg/g isoliquiritigenin 0.2321mg/g, 0.2619mg/g glycyrrhizin and 47.93mg glycyrrhizic acid; it can be seen that the content of the effective components of the white peony root is obviously reduced.
In the step 1) in the comparative example 3, only 85wt% of ethanol aqueous solution is replaced by 60wt% of ethanol aqueous solution, the obtained 6.58g of radix paeoniae alba and licorice soup freeze-dried powder is marked as DM3, the dry paste rate is 27.38%, and the radix paeoniae alba and licorice soup freeze-dried powder DM3 contains 1.0123mg/g gallic acid, 3.327mg/g isoliquiritigenin, 0.0041mg/g paeonol, 0.8264mg of paeoniflorin, 38.71mg/g paeoniflorin, 0.9153mg/g paeoniflorin, 0.0375mg/g benzoic acid, 0.1497mg/g naringenin, 2.524mg/g benzoylpaeoniflorin, 28.72mg/g apigenin, 25.98mg/g glycyrrhizin, 0.1231mg/g formononetin, 0.1042mg/g neoglycyrrhizin, 0.1410mg/g 3' -deoxysappan, 0.2306mg isoliquiritigenin, 0.2617mg/g and 48.04mg glycyrrhizic acid; it can be seen that the content of part of the effective components in the white paeony root is obviously reduced.
In the step 1) of the comparative example 4, the pH value is not adjusted, the obtained 6.72g of the freeze-dried powder of the Paeonia lactiflora decoction is directly soaked in an ethanol aqueous solution, the dry paste rate is 28.00 percent, and the DM4 of the Paeonia lactiflora decoction contains 1.845mg/g gallic acid, 3.321mg/g isoliquiritigenin, 0.0047mg/g paeonol, 1.126mg/g paeoniflorin, 32.69mg/g paeoniflorin, 0.0824mg/g paeoniflorin B, 0.0563mg/g benzoic acid, 0.1392mg/g naringenin, 4.524mg/g benzoyl paeoniflorin, 28.69mg/g apioglycoside, 25.94mg/g glycyrrhizin, 0.1236mg/g formononetin, 0.1029mg/g neoglycyrrhizin, 3' -deoxy Su Mutong A0.1419 mg/g, 0.2324mg isoliquiritigenin 0.2626mg/g and 47.85mg glycyrrhizic acid; it can be seen that the content of part of the effective components in the white paeony root is obviously reduced.
In the step 1) of the comparative example 5, the obtained 7.09g of freeze-dried powder of the peony licorice soup, marked as DM5, has a dry paste rate of 29.54%, and the freeze-dried powder DM5 of the peony licorice soup contains 2.076mg/g gallic acid, 3.325mg/g isoliquiritigenin, 0.0007mg/g paeonol, 1.321mg/g albiflorin, 49.69mg/g paeoniflorin, 0.1034mg/g albiflorin B, 0.0667mg/g benzoic acid, 0.1534mg/g naringenin, 5.521mg/g benzoylpaeoniflorin, 28.72mg/g apioglycoside, 26.21mg/g glycyrrhizin, 0.1214mg/g formononetin, 0.1039mg/g neoglycyrrhizin, 3' -deoxy Su Mutong A0.1424 mg/g isoliquiritigenin, 0.2316mg/g isoliquiritigenin, 0.2625mg/g glycyrrhizin and 47.91mg/g glycyrrhizic acid; it can be seen that the content of paeonol and other effective components in the white paeony root is obviously reduced.
In the step 2) of the comparative example 6, the pH value is not regulated, water is directly added for soaking, the obtained 6.96g of freeze-dried powder of the peony licorice soup is marked as DM6, the dry paste rate is 29.00 percent, and the freeze-dried powder DM6 of the peony licorice soup contains 2.076mg/g gallic acid, 2.672mg/g isoliquiritigenin, 0.0057mg/g paeonol, 1.364mg/g albiflorin, 52.68mg/g paeoniflorin, 0.1026mg/g albiflorin B, 0.0678mg/g benzoic acid, 0.1524mg naringenin, 5.531mg/g benzoyl paeoniflorin, 22.92mg/g apioside, 20.71mg/g glycyrrhizin, 0.0954mg of formononetin, 0.0623mg/g neoglycyrrhizin, 0.0324mg/g 3' -deoxidized Su Mutong A, 0.1059mg isoliquiritigenin, 0.1379mg/g glycyrrhizin and 26.15mg/g glycyrrhizic acid; it can be seen that the content of the effective components in the licorice root is obviously reduced.
It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Claims (9)
1. The preparation method of the freeze-dried powder of the peony and licorice soup is characterized by comprising the following steps of:
adding white paeony root into an ethanol water solution with the concentration of 80-90 wt%, regulating the pH value to 6.0-6.5, soaking, covering and decocting, and filtering to obtain white paeony root liquid medicine;
adding licorice into water, adjusting the pH value to 7.2-7.5, soaking, decocting, and filtering to obtain licorice liquid medicine;
mixing radix Paeoniae alba liquid medicine and Glycyrrhrizae radix liquid medicine, concentrating, and lyophilizing to obtain the radix Paeoniae and Glycyrrhrizae radix soup lyophilized powder.
2. The method for preparing freeze-dried powder of paeonia lactiflora and licorice decoction according to claim 1, wherein the dosage of the ethanol aqueous solution is 7-8 times of the weight of the paeonia lactiflora; the water is 8-10 times of the licorice by weight.
3. The method for preparing the freeze-dried powder of the peony and licorice decoction according to claim 1 or 2, wherein the radix paeoniae alba is decocted with slow fire for 1.5-2 hours; the liquorice is decocted for 2-3 hours by slow fire.
4. The method for preparing the freeze-dried powder of the peony and licorice soup according to claim 1 or 2, wherein the soaking time of the radix paeoniae alba and the licorice is 0.5-1 h.
5. The preparation method of the freeze-dried powder of paeonia lactiflora and licorice decoction according to claim 1 or 2, wherein the concentration is carried out under reduced pressure at 60-80 ℃ and-0.08 to-0.1 MPa.
6. The method for preparing the freeze-dried powder of the peony and licorice soup according to claim 1 or 2, wherein the total weight ratio of the concentrated solution to the radix paeoniae alba and the licorice is 1.8-2.2 after concentration and before freeze-drying: 1.
7. the method for preparing the freeze-dried powder of the peony and licorice soup according to claim 1 or 2, wherein the freeze-drying is performed by pre-freezing at-30 to-45 ℃ for at least 60min and then vacuum drying at-40 to-70 ℃ for at least 12h.
8. The method for preparing freeze-dried powder of paeonia lactiflora and licorice decoction according to claim 7, wherein the vacuum degree of vacuum drying is less than 100Pa.
9. The method for preparing the freeze-dried powder of the peony and licorice soup according to claim 1 or 2, wherein the weight ratio of the radix paeoniae alba to the licorice is 1:1.
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| CN113820422A (en) * | 2021-09-24 | 2021-12-21 | 宁波立华制药有限公司 | Method for detecting total glucosides of paeony by fingerprint spectrum |
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